Process for the preparation of phosphorus pentafluoride and apparatus therefor

Abstract

The application provides a preparation method and device of phosphorus pentafluoride, and the preparation method comprises the following steps: 1) performing atomization treatment on a mixed acid solution comprising a hexafluorophosphoric acid solution and a sulfuric acid solution to obtain atomized mixed acid; and 2) performing a thermal cracking reaction on the atomized mixed acid to obtain phosphorus pentafluoride. The preparation method of phosphorus pentafluoride provided by the application can improve the purity of the prepared phosphorus pentafluoride, and has the advantages of high reaction efficiency, simple process and the like.

Description

Technical Field

[0001] This invention relates to a method and apparatus for preparing phosphorus pentafluoride, belonging to the field of chemical material preparation technology. Background Technology

[0002] In industrial applications, the production of phosphorus pentafluoride (PF5) from the interaction of hexafluorophosphoric acid (HPF6) and sulfuric acid is a task involving thermodynamic and kinetic control. Strict control of reaction conditions is required to prevent unintended side reactions and ensure efficient recovery of the target product.

[0003] The current method of reacting hexafluorophosphoric acid with fuming sulfuric acid presents a series of technical challenges and difficulties, such as low product selectivity and numerous byproducts during the reaction, resulting in low yield efficiency and purity of phosphorus pentafluoride.

[0004] Therefore, optimizing reaction conditions to improve the purity of phosphorus pentafluoride, reduce the generation of byproducts, and increase production efficiency are problems that urgently need to be solved by those skilled in the art. Summary of the Invention

[0005] This invention provides a method for preparing phosphorus pentafluoride, which can improve the purity of the prepared phosphorus pentafluoride and has the advantages of high production efficiency and simple process.

[0006] This invention provides an apparatus for preparing phosphorus pentafluoride, which provides excellent conditions for the preparation of phosphorus pentafluoride, thereby achieving the preparation of high-purity phosphorus pentafluoride.

[0007] This invention provides a method for preparing phosphorus pentafluoride, comprising the following steps: 1) Atomize a mixed acid solution containing hexafluorophosphate solution and sulfuric acid solution to obtain atomized mixed acid; 2) The atomized mixed acid is subjected to thermal decomposition reaction to obtain phosphorus pentafluoride.

[0008] In the preparation method of phosphorus pentafluoride as described above, the droplet size in the atomized mixed acid is 5-200 μm.

[0009] In the preparation method of phosphorus pentafluoride as described above, the droplet size in the atomized mixed acid is 60-100 μm.

[0010] In the preparation method of phosphorus pentafluoride as described above, the atomization treatment is ultrasonic atomization treatment, the atomization temperature of the ultrasonic atomization treatment is 30-85℃, the ultrasonic frequency is 1.5-1.7MHz, and the atomization treatment rate is 20-100kg / min.

[0011] In the method for preparing phosphorus pentafluoride as described above, the hexafluorophosphate solution comprises, by mass percentage, 39.5-65% hexafluorophosphate, 25-55.5% hydrofluoric acid, and 5-10% water. The sulfuric acid solution has a mass concentration of over 98%.

[0012] In the method for preparing phosphorus pentafluoride as described above, the mass ratio of the sulfuric acid solution to the hexafluorophosphate solution is 1:(3-1).

[0013] In the preparation method of phosphorus pentafluoride as described above, the thermal decomposition reaction is carried out at a temperature of 120-160°C, a pressure of -0.9-0 MPaG, and a reaction time of 0.1-5 min.

[0014] The method for preparing phosphorus pentafluoride as described above further includes the following steps after step 2): cooling the phosphorus pentafluoride to obtain a first gas phase system, and then separating the first gas phase system to obtain high-purity phosphorus pentafluoride. The water content in the first gas phase system is not higher than 10 ppm by mass.

[0015] In the preparation method of phosphorus pentafluoride as described above, the temperature of the cooling treatment is 20-80°C.

[0016] The method for preparing phosphorus pentafluoride as described above, wherein the separation process includes the following steps: The first gas phase system was subjected to high-pressure and low-temperature treatment, followed by distillation, to obtain the high-purity phosphorus pentafluoride; The high-pressure low-temperature treatment has a pressure of 1-3 MPa and a temperature of -30-20℃, while the distillation treatment has a distillation pressure of 0.7-2.7 MPa and a distillation temperature of -10-20℃.

[0017] The present invention provides an apparatus for preparing phosphorus pentafluoride, comprising an atomization unit and a thermal decomposition unit; The outlet of the atomizing unit is connected to the inlet of the pyrolysis unit.

[0018] The apparatus for preparing phosphorus pentafluoride as described above, wherein the apparatus further includes a cooling unit and a gas phase separation unit; The inlet of the cooling unit is connected to the outlet of the pyrolysis unit, and the outlet of the cooling unit is connected to the inlet of the gas phase separation unit.

[0019] The method for preparing phosphorus pentafluoride provided by this invention involves mixing a hexafluorophosphate solution with a sulfuric acid solution to effectively reduce the water content in the hexafluorophosphate solution. Subsequently, the mixed acid solution is atomized, reducing the droplet size and effectively increasing the heat transfer surface area and reaction contact surface area of ​​the atomized acid droplets during the thermal decomposition reaction. This enhances mass transfer during the thermal decomposition process, significantly improving the efficiency of the thermal decomposition reaction and shortening the reaction time. Simultaneously, thermal decomposition of the atomized mixed acid reduces the occurrence of side reactions, thereby improving the purity of phosphorus pentafluoride.

[0020] The phosphorus pentafluoride preparation apparatus provided by this invention can precisely control the atomization temperature, ultrasonic frequency, atomization volume, and thermal decomposition reaction temperature of the atomization process, so that hexafluorophosphoric acid can be efficiently and rapidly decomposed into phosphorus pentafluoride and hydrogen fluoride after being atomized into small droplets, and the occurrence of side reactions is reduced, thereby achieving the preparation of high-purity phosphorus pentafluoride. Detailed Implementation

[0021] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions in the embodiments of this invention will be clearly and completely described below in conjunction with the embodiments of this invention. Obviously, the described embodiments are only some embodiments of this invention, not all embodiments. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this invention.

[0022] This invention provides a method for preparing phosphorus pentafluoride, comprising the following steps: 1) Atomize a mixed acid solution containing hexafluorophosphate solution and sulfuric acid solution to obtain atomized mixed acid; 2) The atomized mixed acid was subjected to thermal decomposition to obtain phosphorus pentafluoride.

[0023] Specifically, in step 1), the hexafluorophosphate solution and the sulfuric acid solution are mixed to obtain a mixed acid solution, and then the mixed acid solution is atomized to obtain atomized mixed acid.

[0024] The hexafluorophosphate solution comprises, by mass percentage, 39.5-65% hexafluorophosphate, 25-55.5% hydrofluoric acid, and 5-10% water. The sulfuric acid solution has a mass concentration of over 98%.

[0025] The mass ratio of the sulfuric acid solution to hexafluorophosphate is 1:(3-1). The mass ratio of the sulfuric acid solution to hexafluorophosphate can be adjusted according to the specific mass concentration of the sulfuric acid solution and the specific water content of the hexafluorophosphate solution, so that the sulfuric acid solution can effectively react and remove the water from the hexafluorophosphate solution.

[0026] The present invention does not limit the specific parameters of the mixing process; for example, the mixing process can be carried out under stirring conditions.

[0027] This invention does not limit the specific parameters of the atomization process, and can be selected according to actual needs.

[0028] Step 2) involves thermally decomposing the atomized mixed acid obtained in Step 1) to obtain phosphorus pentafluoride.

[0029] This invention does not limit the specific parameters of the thermal decomposition reaction, and can be selected according to actual needs.

[0030] The preparation method of this invention involves mixing hexafluorophosphate solution with sulfuric acid solution to reduce the water content of the hexafluorophosphate solution, which is beneficial for the subsequent thermal decomposition of hexafluorophosphate into phosphorus pentafluoride and hydrogen fluoride. Subsequently, the mixed acid solution is atomized, reducing the droplet size and effectively increasing the heat transfer surface area and reaction contact surface area of ​​the atomized droplets during the thermal decomposition reaction. This enhances mass transfer during the thermal decomposition process, significantly improving the efficiency of the thermal decomposition reaction and shortening the reaction time. Simultaneously, this enhanced micro-scale mixing uniformity ensures a more complete reaction between hexafluorophosphate and sulfuric acid, reducing the formation of byproducts caused by localized overheating or incomplete reactions, particularly undesirable products such as POF3, whose production is effectively controlled, thereby improving the purity of phosphorus pentafluoride.

[0031] In one specific embodiment, the droplet size in the atomized mixed acid is 5-200 μm, for example, the droplet size in the atomized mixed acid is 5 μm, 10 μm, 25 μm, 50 μm, 75 μm, 100 μm, 125 μm, 150 μm, 175 μm, or 200 μm. When the droplet size in the atomized mixed acid is within the above range, the heat transfer surface area and reaction contact surface area of ​​the droplets in the atomized mixed acid can be increased to a greater extent in the thermal decomposition reaction, and the mass transfer effect of the droplets in the atomized mixed acid can be further enhanced, thereby greatly improving the efficiency of the thermal decomposition reaction. At the same time, it can further reduce the occurrence of side reactions in the thermal decomposition reaction, thereby making the purity of phosphorus pentafluoride higher.

[0032] In one specific embodiment, the droplet size in the atomized mixed acid is 60-100 μm, for example, the droplet size in the atomized mixed acid is 60 μm, 65 μm, 70 μm, 75 μm, 80 μm, 85 μm, 90 μm, 95 μm, or 100 μm. When the droplet size in the atomized mixed acid is within the above range, the heat transfer surface area and reaction contact surface area of ​​the droplets in the atomized mixed acid reach a more suitable range, resulting in stronger mass transfer of the droplets. This improves reaction efficiency while minimizing the generation of side reactions, thereby achieving more efficient preparation of high-purity phosphorus pentafluoride.

[0033] In one specific embodiment, the atomization treatment is ultrasonic atomization treatment. The atomization temperature of the ultrasonic atomization treatment is 30-85℃, for example, the atomization temperature is 30℃, 35℃, 40℃, 45℃, 50℃, 55℃, 60℃, 65℃, 70℃, 75℃, 80℃ or 85℃, etc., the ultrasonic frequency is 1.5-1.7MHz, for example, the ultrasonic frequency is 1.5MHz, 1.55MHz, 1.6MHz, 1.65MHz or 1.7MHz, etc., and the atomization treatment rate is 20-100kg / min, for example, the atomization treatment rate is 20kg / min, 30kg / min, 40kg / min, 50kg / min, 60kg / min, 70kg / min, 80kg / min, 90kg / min or 100kg / min, etc. When ultrasonic atomization is selected for atomization and the parameters are controlled within the above range, it is beneficial to control the droplets in the atomized mixed acid within the range of 5-200μm, thereby ensuring the efficient thermal decomposition reaction of the atomized mixed acid, reducing the generation of side reactions in the thermal decomposition reaction, improving the purity of phosphorus pentafluoride, and further accelerating the production speed of phosphorus pentafluoride by increasing the atomization treatment volume, thus avoiding the waste of energy and time caused by low atomization treatment volume.

[0034] In one specific embodiment, the reaction temperature of the thermal decomposition reaction is 120-160℃, for example, the reaction temperature is 120℃, 125℃, 130℃, 135℃, 140℃, 145℃, 150℃, 155℃ or 160℃, etc., the reaction pressure is -0.9-0 MPaG, the reaction pressure is -0.9MPaG, -0.8MPaG, -0.7MPaG, -0.6MPaG, -0.5MPaG, -0.4MPaG, -0.3MPaG, -0.2MPaG, -0.1MPaG or 0, etc., and the reaction time is 0.1-5 min, the reaction time is 0.1 min, 0.5 min, 1 min, 1.5 min, 2 min, 2.5 min, 3 min, 3.5 min, 4 min, 4.5 min or 5 min, etc. When the reaction temperature, reaction pressure, and reaction time of the thermal decomposition reaction are within the above ranges, the hexafluorophosphoric acid in the atomized mixed acid can be rapidly and efficiently decomposed into phosphorus pentafluoride and hydrogen fluoride. It can also reduce the probability of sulfuric acid reacting with hydrofluoric acid to produce impurities such as fluorosulfonic acid, thereby enabling the more efficient preparation of phosphorus pentafluoride with high purity.

[0035] In one specific embodiment, after step 2), the following steps are further included: cooling phosphorus pentafluoride to obtain a first gaseous system, and then separating the first gaseous system to obtain high-purity phosphorus pentafluoride; wherein the mass percentage of water in the first gaseous system is not higher than 10 ppm. The phosphorus pentafluoride obtained after the thermal decomposition reaction contains sulfur trioxide gas and water vapor. During the cooling process, the water vapor reacts with the sulfur trioxide gas to generate liquid sulfuric acid, thereby reducing the water content in the first gaseous system to a level not exceeding 10 ppm, which is beneficial for the application of phosphorus pentafluoride in other battery materials. Furthermore, the cooling process can reduce the side reaction rate between hydrogen fluoride and sulfur trioxide, thereby reducing the content of fluorosulfonic acid in the liquid phase, which is beneficial for the co-production of sulfuric acid and avoids excessive fluorosulfonic acid content in the liquid phase, preventing the sulfuric acid from being unusable in subsequent applications. The subsequent separation process of the first gaseous system can remove hydrogen fluoride and other impurities from the first gaseous system to obtain high-purity phosphorus pentafluoride. The high-purity phosphorus pentafluoride has a purity of over 99.99%, with HF ≤ 25 ppm and moisture ≤ 10 ppm, which is beneficial for its application in other battery materials.

[0036] In one specific embodiment, the cooling temperature is 20-80°C, for example, 20°C, 30°C, 40°C, 50°C, 60°C, 70°C, or 80°C. When the cooling temperature is within the above range, it is beneficial for the reaction of sulfur trioxide with water and can inhibit the reaction of sulfur trioxide with hydrogen fluoride, thereby enabling the water content in the first gas phase system to reach the above range and reducing the probability of impurities generated by side reactions, thus achieving higher purity phosphorus pentafluoride.

[0037] In one specific embodiment, the separation process includes the following steps: subjecting the first gas phase system to high-pressure, low-temperature treatment, followed by distillation, to obtain high-purity phosphorus pentafluoride; wherein the pressure of the high-pressure, low-temperature treatment is 1-3 MPa, for example, 1 MPa, 1.2 MPa, 1.4 MPa, 1.6 MPa, 1.8 MPa, 2 MPa, 2.2 MPa, 2.4 MPa, 2.6 MPa, 2.8 MPa, or 3 MPa, and the temperature is -30-20°C, for example, -30°C, -25°C, -20°C, -15°C, -10°C, -5°C, 0.5°C, 10°C, 15°C, or 20°C, etc. The distillation pressure for the distillation process is 0.7-2.7 MPa, for example, distillation pressures of 0.7 MPa, 0.8 MPa, 0.9 MPa, 1 MPa, 1.1 MPa, 1.2 MPa, 1.3 MPa, 1.4 MPa, 1.5 MPa, 1.6 MPa, 1.7 MPa, 1.8 MPa, 1.9 MPa, 2 MPa, 2.1 MPa, 2.2 MPa, 2.3 MPa, 2.4 MPa, 2.5 MPa, 2.6 MPa, or 2.7 MPa, etc., and the distillation temperature is -10-20℃, for example, distillation temperatures of -10℃, -5℃, 0℃, 5℃, 10℃, 15℃, or 20℃, etc. Specifically, the separation process includes the following steps: The first gas phase system is subjected to high-pressure, low-temperature treatment to transform it into a liquid phase; subsequently, distillation is performed to separate hydrogen fluoride and impurities from phosphorus pentafluoride, yielding a bottom liquid, which is high-purity phosphorus pentafluoride. This separation process effectively separates phosphorus pentafluoride from hydrogen fluoride and other impurities in the first gas phase system, resulting in high-purity phosphorus pentafluoride.

[0038] This invention provides an apparatus for preparing phosphorus pentafluoride, comprising an atomization unit and a pyrolysis unit; wherein the outlet of the atomization unit is connected to the inlet of the pyrolysis unit. The atomization unit and pyrolysis unit provided by this invention can precisely control the atomization temperature, ultrasonic frequency, and atomization volume of the atomization process, thereby producing atomized mixed acid with suitable droplet size. Subsequently, the pyrolysis unit can precisely control the reaction temperature of the pyrolysis reaction, enabling hexafluorophosphoric acid to decompose efficiently and rapidly into phosphorus pentafluoride and hydrogen fluoride, while minimizing the occurrence of side reactions, thus achieving the preparation of high-purity phosphorus pentafluoride.

[0039] In one specific embodiment, the phosphorus pentafluoride preparation apparatus further includes a cooling unit and a gas phase separation unit; wherein, the inlet of the cooling unit is connected to the outlet of the thermal cracking unit, and the outlet of the cooling unit is connected to the inlet of the gas phase separation unit. The phosphorus pentafluoride preparation apparatus, including the cooling unit and the gas phase separation unit, can reduce the moisture content in the phosphorus pentafluoride obtained after the thermal cracking reaction, suppress side reactions, and effectively separate phosphorus pentafluoride from hydrogen fluoride, other impurities, etc., thereby achieving the preparation of high-purity phosphorus pentafluoride.

[0040] The present invention will be further described in detail below through specific embodiments.

[0041] Example 1 The preparation process of phosphorus pentafluoride provided in this embodiment includes the following steps: 1) Mix hexafluorophosphate solution with sulfuric acid solution with a mass percentage of 98% to obtain mixed acid solution, and then perform ultrasonic atomization treatment on the mixed acid solution to obtain atomized mixed acid; The hexafluorophosphate solution comprises 40% hexafluorophosphate, 53% hydrofluoric acid, and 7% water by mass percentage; the mass ratio of hexafluorophosphate solution to sulfuric acid solution is 1:2; the ultrasonic atomization treatment is performed at an atomization temperature of 35℃, an ultrasonic frequency of 1.7MHz, and an atomization rate of 25kg / min; the atomized mixed acid is tested by an aerosol particle size analyzer, and the droplet size in the atomized mixed acid is 70μm.

[0042] 2) The atomized mixed acid is subjected to thermal cracking reaction in a thermal cracking reactor, and then cooled to obtain a first gas phase system. The first gas phase system is then subjected to high pressure and low temperature treatment, and then subjected to distillation to obtain high-purity phosphorus pentafluoride. The thermal decomposition reaction was carried out at a temperature of 130℃, a pressure of -0.9 MPaG, and a time of 5 min. The cooling temperature was 80℃, and the water content in the first gas phase system was 8 ppm by mass. The high-pressure cryogenic treatment has a pressure of 2.5 MPa and a temperature of 10℃, while the distillation treatment has a distillation pressure of 2.3 MPa and a distillation temperature of 20℃.

[0043] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 20 ppm, and the water content was 7 ppm by mass.

[0044] Example 2 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1. The difference is that the atomization temperature of ultrasonic atomization treatment is 32℃, the ultrasonic frequency is 1.68MHz, and the atomization treatment rate is 30kg / min. The atomized mixed acid is tested by an aerosol particle size analyzer, and the droplet size in the atomized mixed acid is 88μm.

[0045] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 19 ppm, and the water content was 7 ppm by mass.

[0046] Example 3 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the atomization temperature of ultrasonic atomization is 32°C, the ultrasonic frequency is 1.5MHz, and the atomization rate is 50kg / min; the atomized mixed acid is tested by an aerosol particle size analyzer, and the droplet size in the atomized mixed acid is 165μm.

[0047] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 24 ppm, and the water content was 8 ppm by mass.

[0048] Example 4 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1. The difference is that the atomization temperature of ultrasonic atomization treatment is 25°C, the ultrasonic frequency is 1.4MHz, and the atomization treatment rate is 110kg / min. The atomized mixed acid was tested by an aerosol particle size analyzer, and the droplet size in the atomized mixed acid was 189μm.

[0049] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.98%, the HF content was 60 ppm, and the water content was 8 ppm by mass.

[0050] Example 5 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1. The difference is that the atomization temperature of ultrasonic atomization is 25°C, the ultrasonic frequency is 1.41MHz, and the atomization rate is 110kg / min. The atomized mixed acid is tested by an aerosol particle size analyzer, and the droplet size in the atomized mixed acid is 250μm.

[0051] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.96%, the HF content was 260 ppm, and the water content was 8 ppm by mass.

[0052] Example 6 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1. The difference is that the atomization temperature of the ultrasonic atomization treatment is 30°C, the ultrasonic frequency is 1.7MHz, and the atomization treatment rate is 20kg / min. The atomized mixed acid is tested by an aerosol particle size analyzer, and the droplet size in the atomized mixed acid is 30μm.

[0053] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 19 ppm, and the water content was 7 ppm by mass.

[0054] Example 7 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1. The difference is that the atomization temperature of ultrasonic atomization treatment is 50°C, the ultrasonic frequency is 1.6MHz, and the atomization treatment rate is 50kg / min. The atomized mixed acid is tested by an aerosol particle size analyzer, and the droplet size in the atomized mixed acid is 60μm.

[0055] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 20 ppm, and the water content was 7 ppm by mass.

[0056] Example 8 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the atomization temperature of ultrasonic atomization is 60℃, the ultrasonic frequency is 1.5MHz, and the atomization rate is 50kg / min; the atomized mixed acid is tested by an aerosol particle size analyzer, and the droplet size in the atomized mixed acid is 100μm.

[0057] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 23 ppm, and the water content was 8 ppm by mass.

[0058] Example 9 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1. The difference is that the atomization temperature of the ultrasonic atomization treatment is 80℃, the ultrasonic frequency is 1.5MHz, and the atomization treatment rate is 80kg / min. The atomized mixed acid is tested by an aerosol particle size analyzer, and the droplet size in the atomized mixed acid is 88μm.

[0059] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 22 ppm, and the water content was 7 ppm by mass.

[0060] Example 10 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1. The difference is that the atomization temperature of ultrasonic atomization treatment is 90℃, the ultrasonic frequency is 1.3MHz, and the atomization treatment rate is 100kg / min. The atomized mixed acid is tested by an aerosol particle size analyzer, and the droplet size in the atomized mixed acid is 30μm.

[0061] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 55 ppm, and the water content was 8 ppm by mass.

[0062] Example 11 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the reaction temperature of the thermal decomposition reaction is 140°C, the reaction pressure is -0.95 MPaG, and the reaction time is 1 min.

[0063] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 29 ppm, and the water content was 8 ppm by mass.

[0064] Example 12 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the reaction temperature of the thermal decomposition reaction is 145°C, the reaction pressure is -0.95 MPaG, and the reaction time is 5 min.

[0065] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 25 ppm, and the water content was 8 ppm by mass.

[0066] Example 13 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the reaction temperature of the thermal decomposition reaction is 110°C, the reaction pressure is 0.1 MPaG, and the reaction time is 10 min.

[0067] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.92%, the HF content was 500 ppm, and the water content was 8 ppm by mass.

[0068] Example 14 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the reaction temperature of the thermal decomposition reaction is 120°C, the reaction pressure is -0.7 MPaG, and the reaction time is 0.1 min.

[0069] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 28 ppm, and the water content was 8 ppm by mass.

[0070] Example 15 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the reaction temperature of the thermal decomposition reaction is 140°C, the reaction pressure is -0.5 MPaG, and the reaction time is 1 min.

[0071] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 25 ppm, and the water content was 7 ppm by mass.

[0072] Example 16 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the reaction temperature of the thermal decomposition reaction is 160°C, the reaction pressure is -0.3 MPaG, and the reaction time is 3 min.

[0073] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 21 ppm, and the water content was 7 ppm by mass.

[0074] Example 17 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the cooling temperature is 60°C and the mass percentage of water in the first gas phase system is 9 ppm.

[0075] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 20 ppm, and the water content was 8 ppm by mass.

[0076] Example 18 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the cooling temperature is 50°C and the mass percentage of water in the first gas phase system is 10 ppm.

[0077] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 24 ppm, and the water content was 9 ppm by mass.

[0078] Example 19 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the cooling temperature is 20°C and the mass percentage of water in the first gas phase system is 10 ppm.

[0079] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 24 ppm, and the water content was 9 ppm by mass.

[0080] Example 20 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the cooling temperature is 10°C and the mass percentage of water in the first gas phase system is 10 ppm.

[0081] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 30 ppm, and the water content was 9 ppm by mass.

[0082] Example 21 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the cooling temperature is 90°C and the mass percentage of water in the first gas phase system is 13 ppm.

[0083] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.97%, the HF content was 45 ppm, and the water content was 12 ppm by mass.

[0084] Example 22 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the pressure of the high-pressure low-temperature treatment is 2 MPa and the temperature is 8°C, and the distillation pressure of the distillation treatment is 1.8 MPa and the distillation temperature is 10°C.

[0085] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 18 ppm, and the water content was 6 ppm by mass.

[0086] Example 23 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the pressure of the high-pressure low-temperature treatment is 1.5 MPa and the temperature is -7°C, and the distillation pressure of the distillation treatment is 1.2 MPa and the distillation temperature is 0°C.

[0087] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 20 ppm, and the water content was 10 ppm by mass.

[0088] Example 24 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the pressure of the high-pressure low-temperature treatment is 0.9 MPa and the temperature is -37°C, and the distillation pressure of the distillation treatment is 0.7 MPa and the distillation temperature is -25°C.

[0089] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.95%, the HF content was 35 ppm, and the water content was 11 ppm by mass.

[0090] Example 25 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the pressure of the high-pressure low-temperature treatment is 1 MPa and the temperature is -30°C, and the distillation pressure of the distillation treatment is 0.7 MPa and the distillation temperature is -10°C.

[0091] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 21 ppm, and the water content was 9 ppm by mass.

[0092] Example 26 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the pressure of the high-pressure low-temperature treatment is 3 MPa and the temperature is 20°C, and the distillation pressure of the distillation treatment is 2.7 MPa and the distillation temperature is 20°C.

[0093] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 21 ppm, and the water content was 9 ppm by mass.

[0094] Example 27 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the hexafluorophosphoric acid solution includes hexafluorophosphoric acid 39.5%, hydrofluoric acid 55.5%, and water 5% by mass percentage.

[0095] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 24 ppm, and the water content was 7 ppm by mass.

[0096] Example 28 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the hexafluorophosphoric acid solution includes 50% hexafluorophosphoric acid, 45% hydrofluoric acid, and 5% water by mass percentage.

[0097] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 20 ppm, and the water content was 7 ppm by mass.

[0098] Example 29 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the hexafluorophosphoric acid solution includes 65% hexafluorophosphoric acid, 25% hydrofluoric acid, and 10% water by mass percentage.

[0099] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 18 ppm, and the water content was 8 ppm by mass.

[0100] Example 30 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the hexafluorophosphate solution includes 38% hexafluorophosphate, 58% hydrofluoric acid, and 4% water by mass percentage.

[0101] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.98%, the HF content was 38 ppm, and the water content was 7 ppm by mass.

[0102] Example 31 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the mass percentage of sulfuric acid solution is 100%.

[0103] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 20 ppm, and the water content was 7 ppm by mass.

[0104] Example 32 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the mass percentage of sulfuric acid solution is 97%.

[0105] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.98%, the HF content was 35 ppm, and the water content was 10 ppm by mass.

[0106] Example 33 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the mass ratio of hexafluorophosphate solution to sulfuric acid solution is 1:1.

[0107] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 19 ppm, and the water content was 7 ppm by mass.

[0108] Example 34 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the mass ratio of hexafluorophosphate solution to sulfuric acid solution is 1:3.

[0109] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.99%, the HF content was 23 ppm, and the water content was 7 ppm by mass.

[0110] Example 35 The preparation process of phosphorus pentafluoride provided in this embodiment is roughly the same as that in Example 1, except that the mass ratio of hexafluorophosphate solution to sulfuric acid solution is 1:4.

[0111] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.98%, the HF content was 33 ppm, and the water content was 11 ppm by mass.

[0112] Example 36 The preparation process of phosphorus pentafluoride provided in this embodiment includes the following steps: 1) Mix hexafluorophosphate solution with sulfuric acid solution with a mass percentage of 98% to obtain mixed acid solution, and then perform ultrasonic atomization treatment on the mixed acid solution to obtain atomized mixed acid; The hexafluorophosphate solution comprises 40% hexafluorophosphate, 53% hydrofluoric acid, and 7% water by mass percentage; the mass ratio of hexafluorophosphate solution to sulfuric acid solution is 1:2; the ultrasonic atomization treatment has an atomization temperature of 35℃, an ultrasonic frequency of 1.7MHz, and an atomization rate of 25kg / min; the droplet size in the atomized mixed acid is 70μm.

[0113] 2) The atomized mixed acid is subjected to thermal pyrolysis in a thermal pyrolysis reactor to obtain a phosphorus pentafluoride mixed gas; The thermal decomposition reaction was carried out at a temperature of 130℃, a pressure of -0.9 MPaG, and a time of 5 min.

[0114] GC-MS and online infrared spectroscopy tests on the phosphorus pentafluoride mixture revealed that the phosphorus pentafluoride purity was 70.70%, the HF content was 29.30%, and the moisture content was 12 ppm.

[0115] Example 37 The preparation process of phosphorus pentafluoride provided in this embodiment includes the following steps: 1) Mix hexafluorophosphate solution with sulfuric acid solution with a mass percentage of 98% to obtain mixed acid solution, and then perform ultrasonic atomization treatment on the mixed acid solution to obtain atomized mixed acid; The hexafluorophosphate solution comprises 40% hexafluorophosphate, 53% hydrofluoric acid, and 7% water by mass percentage; the mass ratio of hexafluorophosphate solution to sulfuric acid solution is 1:2; the ultrasonic atomization treatment has an atomization temperature of 32℃, an ultrasonic frequency of 1.68MHz, and an atomization rate of 30kg / min; the droplet size in the atomized mixed acid is 88μm.

[0116] 2) The atomized mixed acid is subjected to thermal decomposition reaction to obtain a phosphorus pentafluoride mixed gas; The thermal decomposition reaction was carried out at a temperature of 130℃, a pressure of -0.9 MPaG, and a time of 5 min.

[0117] GC-MS and online infrared spectroscopy tests on the phosphorus pentafluoride mixture showed that the purity of phosphorus pentafluoride was 69.60%, the HF content was 30.39%, and the water content was 13 ppm.

[0118] Example 38 The preparation process of phosphorus pentafluoride provided in this embodiment includes the following steps: 1) Mix hexafluorophosphate solution with sulfuric acid solution with a mass percentage of 98% to obtain mixed acid solution, and then perform ultrasonic atomization treatment on the mixed acid solution to obtain atomized mixed acid; The hexafluorophosphate solution comprises 40% hexafluorophosphate, 53% hydrofluoric acid, and 7% water by mass percentage; the mass ratio of hexafluorophosphate solution to sulfuric acid solution is 1:2; the ultrasonic atomization treatment has an atomization temperature of 32℃, an ultrasonic frequency of 1.5MHz, and an atomization rate of 50kg / min; the droplet size in the atomized mixed acid is 165μm.

[0119] 2) The atomized mixed acid is subjected to thermal decomposition reaction to obtain a phosphorus pentafluoride mixed gas; The thermal decomposition reaction was carried out at a temperature of 130℃, a pressure of -0.9 MPaG, and a time of 5 min.

[0120] GC-MS and online infrared spectroscopy tests on the phosphorus pentafluoride mixture showed that the purity of phosphorus pentafluoride was 66.70%, the HF content was 33.28%, and the water content was 15 ppm.

[0121] Example 39 The preparation process of phosphorus pentafluoride provided in this embodiment includes the following steps: 1) Mix hexafluorophosphate solution with sulfuric acid solution with a mass percentage of 98% to obtain mixed acid solution, and then perform ultrasonic atomization treatment on the mixed acid solution to obtain atomized mixed acid; The hexafluorophosphate solution comprises 40% hexafluorophosphate, 53% hydrofluoric acid, and 7% water by mass percentage; the mass ratio of hexafluorophosphate solution to sulfuric acid solution is 1:2; the ultrasonic atomization treatment has an atomization temperature of 35℃, an ultrasonic frequency of 1.7MHz, and an atomization rate of 25kg / min; the droplet size in the atomized mixed acid is 70μm.

[0122] 2) The atomized mixed acid is subjected to thermal decomposition in a thermal decomposition reactor, followed by cooling treatment to obtain phosphorus pentafluoride; The thermal decomposition reaction was carried out at a temperature of 130℃, a pressure of -0.9 MPaG, and a time of 5 min; the cooling temperature was 80℃.

[0123] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of phosphorus pentafluoride was 90.56%, the HF content was 9.43%, and the water content was 13 ppm.

[0124] Example 40 The preparation process of phosphorus pentafluoride provided in this embodiment includes the following steps: 1) Mix a 40% hexafluorophosphate solution with a 98% sulfuric acid solution to obtain a mixed acid solution. Then, subject the mixed acid solution to ultrasonic atomization to obtain atomized mixed acid. The ultrasonic atomization treatment had an atomization temperature of 32℃, an ultrasonic frequency of 1.68MHz, and an atomization rate of 30kg / min; the droplet size in the atomized mixed acid was 88μm.

[0125] 2) The atomized mixed acid is subjected to thermal decomposition reaction, followed by cooling treatment to obtain phosphorus pentafluoride; The thermal decomposition reaction was carried out at a temperature of 130℃, a pressure of -0.9 MPaG, and a time of 5 min; the cooling temperature was 80℃.

[0126] GC-MS and online infrared spectroscopy tests showed that the purity of phosphorus pentafluoride was 89.78%, the HF content was 10.22%, and the moisture content was 14 ppm.

[0127] Example 41 The preparation process of phosphorus pentafluoride provided in this embodiment includes the following steps: 1) Mix hexafluorophosphate solution with sulfuric acid solution with a mass percentage of 98% to obtain mixed acid solution, and then perform ultrasonic atomization treatment on the mixed acid solution to obtain atomized mixed acid; The hexafluorophosphate solution comprises 40% hexafluorophosphate, 53% hydrofluoric acid, and 7% water by mass percentage; the mass ratio of hexafluorophosphate solution to sulfuric acid solution is 1:2; the ultrasonic atomization treatment has an atomization temperature of 32℃, an ultrasonic frequency of 1.5MHz, and an atomization rate of 50kg / min; the droplet size in the atomized mixed acid is 165μm.

[0128] 2) The atomized mixed acid is subjected to thermal decomposition reaction, followed by cooling treatment to obtain phosphorus pentafluoride; The thermal decomposition reaction was carried out at a temperature of 130℃, a pressure of -0.9 MPaG, and a time of 5 min; the cooling temperature was 80℃.

[0129] GC-MS and online infrared spectroscopy tests showed that the purity of phosphorus pentafluoride was 88.74%, the HF content was 11.75%, and the moisture content was 15 ppm.

[0130] Comparative Example 1 The preparation process of phosphorus pentafluoride provided in this comparative example includes the following steps: A solution of hexafluorophosphate was mixed with a sulfuric acid solution of 98% by mass, and then subjected to thermal cracking reaction. After cooling, a first gas phase system was obtained. Finally, the first gas phase system was subjected to high-pressure and low-temperature treatment, and then subjected to distillation to obtain high-purity phosphorus pentafluoride. The hexafluorophosphate solution comprises 40% hexafluorophosphate, 53% hydrofluoric acid, and 7% water by mass percentage; the mass ratio of hexafluorophosphate solution to sulfuric acid solution is 1:2; the thermal decomposition reaction temperature is 130℃, the reaction pressure is -0.9MPaG, and the reaction time is 5min. The cooling temperature was 80℃, and the water content in the first gas phase system was 8 ppm by mass. The high-pressure cryogenic treatment has a pressure of 2.5 MPa and a temperature of 10℃, while the distillation treatment has a distillation pressure of 2.3 MPa and a distillation temperature of 20℃.

[0131] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 99.10%, the HF content was 520 ppm, and the water content was 8 ppm by mass.

[0132] Comparative Example 2 The preparation process of phosphorus pentafluoride provided in this comparative example includes the following steps: The hexafluorophosphoric acid solution was subjected to thermal cracking reaction, followed by cooling to obtain the first gas phase system. Finally, the first gas phase system was subjected to high pressure and low temperature treatment, followed by distillation to obtain high-purity phosphorus pentafluoride. The hexafluorophosphoric acid solution comprises 40% hexafluorophosphoric acid, 53% hydrofluoric acid, and 7% water by mass percentage; the thermal decomposition reaction temperature is 130℃, the reaction pressure is -0.9MPaG, and the reaction time is 5min. The cooling temperature was 80℃, and the water content in the first gas phase system was 8 ppm by mass. The high-pressure cryogenic treatment has a pressure of 2.5 MPa and a temperature of 10℃, while the distillation treatment has a distillation pressure of 2.3 MPa and a distillation temperature of 20℃.

[0133] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 90.20%, the HF content was 3520 ppm, and the water content was 8 ppm by mass.

[0134] Comparative Example 3 The preparation process of phosphorus pentafluoride provided in this comparative example includes the following steps: 1) The hexafluorophosphate solution was subjected to ultrasonic atomization to obtain atomized hexafluorophosphate; The hexafluorophosphate solution comprises 40% hexafluorophosphate, 53% hydrofluoric acid, and 7% water by mass percentage; the ultrasonic atomization treatment has an atomization temperature of 35℃, an ultrasonic frequency of 1.7MHz, and an atomization rate of 25kg / min; the droplet size in the atomized mixed acid is 70μm.

[0135] 2) The atomized hexafluorophosphoric acid was subjected to thermal decomposition reaction, and then cooled to obtain the first gas phase system. Subsequently, the first gas phase system was subjected to high pressure and low temperature treatment, and then distilled to obtain high-purity phosphorus pentafluoride. The thermal decomposition reaction was carried out at a temperature of 130℃, a pressure of -0.9 MPaG, and a time of 5 min. The cooling temperature was 80℃, and the water content in the first gas phase system was 8 ppm by mass. The high-pressure cryogenic treatment has a pressure of 2.5 MPa and a temperature of 10℃, while the distillation treatment has a distillation pressure of 2.3 MPa and a distillation temperature of 20℃.

[0136] GC-MS and online infrared spectroscopy tests on high-purity phosphorus pentafluoride showed that the purity of high-purity phosphorus pentafluoride was 96.50%, the HF content was 1534 ppm, and the water content was 8 ppm by mass.

[0137] Comparative Example 4 The preparation process of phosphorus pentafluoride provided in this comparative example includes the following steps: A solution of hexafluorophosphoric acid was mixed with a sulfuric acid solution of 98% by mass, and then subjected to a thermal decomposition reaction to obtain a mixed gas of high phosphorus pentafluoride. The hexafluorophosphate solution comprises 40% hexafluorophosphate, 53% hydrofluoric acid, and 7% water by mass percentage; the mass ratio of hexafluorophosphate solution to sulfuric acid solution is 1:2; the thermal decomposition reaction temperature is 130℃, the reaction pressure is -0.9MPaG, and the reaction time is 5min.

[0138] GC-MS and online infrared spectroscopy tests on the phosphorus pentafluoride mixture showed that the purity of phosphorus pentafluoride was 65.50%, the HF content was 34.49%, and the water content was 15 ppm.

[0139] Comparative Example 5 The preparation process of phosphorus pentafluoride provided in this comparative example includes the following steps: A solution of hexafluorophosphate was subjected to thermal decomposition to obtain a mixture of phosphorus pentafluoride gas; The hexafluorophosphate solution comprises 40% hexafluorophosphate, 53% hydrofluoric acid, and 7% water by mass percentage; the thermal decomposition reaction temperature is 130℃, the reaction pressure is -0.9MPaG, and the reaction time is 5min.

[0140] GC-MS and online infrared spectroscopy tests on the phosphorus pentafluoride mixture revealed that the phosphorus pentafluoride purity was 45.50%, the HF content was 51.20%, and the water content was 33,000 ppm.

[0141] Comparative Example 6 The preparation process of phosphorus pentafluoride provided in this comparative example includes the following steps: 1) The hexafluorophosphate solution was subjected to ultrasonic atomization to obtain atomized hexafluorophosphate; The hexafluorophosphate solution comprises 40% hexafluorophosphate, 53% hydrofluoric acid, and 7% water by mass percentage; the ultrasonic atomization treatment has an atomization temperature of 35℃, an ultrasonic frequency of 1.7MHz, and an atomization rate of 25kg / min; the droplet size in the atomized mixed acid is 70μm.

[0142] 2) The atomized hexafluorophosphoric acid was subjected to a thermal decomposition reaction to obtain a mixed gas of phosphorus pentafluoride; The thermal decomposition reaction was carried out at a temperature of 130℃, a pressure of -0.9 MPaG, and a time of 5 min.

[0143] GC-MS and online infrared spectroscopy tests on the phosphorus pentafluoride mixture showed that the purity of phosphorus pentafluoride was 57.20%, the HF content in high-purity phosphorus pentafluoride was 39.70%, and the water content was 31,000 ppm by mass.

[0144] Comparative Example 7 The preparation process of phosphorus pentafluoride provided in this comparative example includes the following steps: A solution of hexafluorophosphate was mixed with a 98% sulfuric acid solution, and then subjected to a thermal decomposition reaction, followed by cooling, to obtain phosphorus pentafluoride. The hexafluorophosphate solution comprises 40% hexafluorophosphate, 53% hydrofluoric acid, and 7% water by mass percentage; the mass ratio of hexafluorophosphate solution to sulfuric acid solution is 1:2; the thermal decomposition reaction temperature is 130℃, the reaction pressure is -0.9MPaG, and the reaction time is 5min; the cooling temperature is 80℃.

[0145] GC-MS and online infrared spectroscopy tests on phosphorus pentafluoride showed that the purity of phosphorus pentafluoride was 74.50%, the HF content was 25.49%, and the moisture content was 15 ppm.

[0146] Comparative Example 8 The preparation process of phosphorus pentafluoride provided in this comparative example includes the following steps: Hexafluorophosphoric acid solution was subjected to thermal decomposition reaction, followed by cooling treatment to obtain phosphorus pentafluoride; The hexafluorophosphoric acid solution comprises 40% hexafluorophosphoric acid, 53% hydrofluoric acid, and 7% water by mass percentage; the thermal decomposition reaction temperature is 130℃, the reaction pressure is -0.9MPaG, and the reaction time is 5min; the cooling treatment temperature is 80℃.

[0147] GC-MS and online infrared spectroscopy tests on phosphorus pentafluoride showed that the purity of phosphorus pentafluoride was 52.10%, the HF content was 45.45%, and the water content was 24,500 ppm.

[0148] Comparative Example 9 The preparation process of phosphorus pentafluoride provided in this comparative example includes the following steps: 1) The hexafluorophosphate solution was subjected to ultrasonic atomization to obtain atomized hexafluorophosphate; The hexafluorophosphate solution comprises 40% hexafluorophosphate, 53% hydrofluoric acid, and 7% water by mass percentage; the ultrasonic atomization treatment has an atomization temperature of 35℃, an ultrasonic frequency of 1.7MHz, and an atomization rate of 25kg / min; the droplet size in the atomized mixed acid is 70μm.

[0149] 2) The atomized hexafluorophosphoric acid is subjected to thermal decomposition reaction, followed by cooling treatment to obtain phosphorus pentafluoride; The thermal decomposition reaction was carried out at a temperature of 130℃, a pressure of -0.9 MPaG, and a time of 5 min; the cooling temperature was 80℃.

[0150] GC-MS and online infrared spectroscopy tests on phosphorus pentafluoride showed that the purity of phosphorus pentafluoride was 66.20%, the HF content was 31.70%, and the water content was 21,000 ppm.

[0151] In summary, as demonstrated by Examples 1-41 and Comparative Examples 1-9, this invention can improve the purity of phosphorus pentafluoride by controlling the parameters of atomization and thermal decomposition treatments. Furthermore, by controlling the parameters of cooling and separation treatments, the purity of high-purity phosphorus pentafluoride can reach 99.99%, with HF content as low as 18 ppm and moisture content as low as 6 ppm. Therefore, the phosphorus pentafluoride preparation method provided by this invention can improve the purity of phosphorus pentafluoride, and the method is highly efficient and simple.

[0152] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing phosphorus pentafluoride, characterized in that, Includes the following steps: 1) Atomize a mixed acid solution containing hexafluorophosphate solution and sulfuric acid solution to obtain atomized mixed acid; 2) The atomized mixed acid is subjected to a thermal decomposition reaction to obtain phosphorus pentafluoride; The droplet size in the atomized mixed acid is 5~200μm; The atomization treatment is ultrasonic atomization treatment, the atomization temperature of the ultrasonic atomization treatment is 30~85℃, the ultrasonic frequency is 1.5~1.7MHz, and the atomization treatment rate is 20~100kg / min; The hexafluorophosphate solution comprises, by mass percentage, 39.5%–65% hexafluorophosphate, 25%–55.5% hydrofluoric acid, and 5%–10% water. The sulfuric acid solution has a mass concentration higher than 98%. The mass ratio of the sulfuric acid solution to the hexafluorophosphate solution is 1:(3~1). The thermal decomposition reaction is carried out at a temperature of 120~160℃, a pressure of -0.9~0MPaG, and a time of 0.1~5min. Step 2) is followed by the following steps: cooling the phosphorus pentafluoride to obtain a first gas phase system, and then separating the first gas phase system to obtain high-purity phosphorus pentafluoride; Wherein, the mass percentage of water in the first gas phase system is not higher than 10 ppm; The cooling temperature is 20~80℃; The separation process includes the following steps: The first gas phase system was subjected to high-pressure and low-temperature treatment, followed by distillation, to obtain the high-purity phosphorus pentafluoride; The high-pressure low-temperature treatment has a pressure of 1~3MPa and a temperature of -30~20℃, and the distillation treatment has a distillation pressure of 0.7~2.7MPa and a distillation temperature of -10~20℃.

2. The method for preparing phosphorus pentafluoride according to claim 1, characterized in that, The droplet size in the atomized mixed acid is 60-100 μm.